CN116813362A - Low-carbon magnesia carbon brick for refining ladle and preparation method thereof - Google Patents
Low-carbon magnesia carbon brick for refining ladle and preparation method thereof Download PDFInfo
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- CN116813362A CN116813362A CN202311110824.XA CN202311110824A CN116813362A CN 116813362 A CN116813362 A CN 116813362A CN 202311110824 A CN202311110824 A CN 202311110824A CN 116813362 A CN116813362 A CN 116813362A
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 174
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 118
- 239000011449 brick Substances 0.000 title claims abstract description 91
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 87
- 238000007670 refining Methods 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000010439 graphite Substances 0.000 claims abstract description 78
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 78
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052796 boron Inorganic materials 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000005011 phenolic resin Substances 0.000 claims abstract description 25
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000002131 composite material Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 8
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 8
- 239000001095 magnesium carbonate Substances 0.000 claims description 8
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 8
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 22
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 230000002829 reductive effect Effects 0.000 abstract description 4
- 239000011819 refractory material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 230000003628 erosive effect Effects 0.000 description 7
- 239000002893 slag Substances 0.000 description 6
- 230000035515 penetration Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- RWDBMHZWXLUGIB-UHFFFAOYSA-N [C].[Mg] Chemical compound [C].[Mg] RWDBMHZWXLUGIB-UHFFFAOYSA-N 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000008354 tissue degradation Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/402—Aluminium
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Abstract
The invention belongs to the technical field of refractory materials, and particularly relates to a low-carbon magnesia carbon brick for a refining ladle and a preparation method thereof. The low-carbon magnesia carbon brick for the refining ladle comprises the following preparation raw materials in parts by mass: 60-90 parts of fused magnesia, 1-10 parts of aluminum powder and 1-5 parts of boron doped ZrO 2 5-10 parts of SiC powder and 1-5 parts of phenolic resin. The invention adopts boron and ZrO 2 The flake graphite is modified to form a three-dimensional network structure, so that a sufficient graphite internal space can be created, the full contact of the graphite and other components is promoted, the function maximization under the low-carbon premise is realized, meanwhile, the stability of the graphite structure can be enhanced, the oxidation rate of the graphite is reduced, and the low-carbon magnesia carbon brick with excellent thermal shock resistance stability and long service life is obtained.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a low-carbon magnesia carbon brick for a refining ladle and a preparation method thereof.
Background
The magnesia carbon brick is a carbon composite refractory material with excellent characteristics of graphite and magnesia, has excellent erosion resistance and thermal shock resistance, and is widely used as a furnace lining material on refined steel ladle.
The carbon material commonly used in magnesia carbon bricks is mainly crystalline flake graphite. The unique lamellar structure of the flake graphite is easy to generate elastic effect in the direction parallel to the forming pressure direction of the brick body, so that the brick body structure is subjected to spalling and heat transfer anisotropy, internal stress concentration of the brick body is caused, and the structural damage of the brick body is accelerated; and the oxidation-easy performance of the crystalline flake graphite is easy to cause oxidation and decarbonization of the surface layer of the magnesia carbon brick, so that the surface layer structure of the brick body is deteriorated, and the erosion resistance and the stripping resistance of the brick body are reduced. In addition, the flake graphite has obvious carburetion effect on molten steel, and is not suitable for smelting low-carbon steel and clean steel.
In the prior art, the carbon content in magnesia carbon bricks is reduced to alleviate the problems, but the reduction of thermal shock stability and slag penetration resistance is brought along with the reduction, the service life is shortened, and the requirements of ladle refining production cannot be completely met. Therefore, it is important to explore how to realize excellent thermal shock stability and long service life of magnesia carbon bricks under the condition of low carbon.
Disclosure of Invention
Aiming at the problems of poor thermal shock resistance stability and short service life of the low-carbon magnesia carbon brick for the refining ladle in the prior art, the invention provides the low-carbon magnesia carbon brick for the refining ladle, which adopts boron and ZrO 2 The flake graphite is modified to form a three-dimensional network structure, so that a sufficient graphite internal space can be created, the full contact of the graphite and other components is promoted, the function maximization under the low-carbon premise is realized, meanwhile, the stability of the graphite structure can be enhanced, the oxidation rate of the graphite is reduced, and the excellent thermal shock resistance stability and long service life are obtained.
The invention provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 60-90 parts of fused magnesia, 1-10 parts of aluminum powder and 1-5 parts of boron doped ZrO 2 5-10 parts of SiC powder and 1-5 parts of phenolic resin;
the boron doped ZrO 2 The preparation method of the graphite composite material comprises the following steps:
s1: soaking the flake graphite in a mixed solution of ethylenediamine and ammonia water for full activation, filtering the flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O) and borate are dissolved in deionized water to form a modified solution; dispersing activated crystalline flake graphite in the modified solution, heating and stirring, filtering, washing with water, and drying to obtain boron doped ZrO 2 Graphite composite material.
Wherein, the ethylenediamine and the ammonia water treatment play roles of surface activation and introducing C-N functional groups, so that the surface of the crystalline flake graphite is promoted to present a microporous hole structure, the subsequent deep modification treatment is more facilitated, the ammonia water can also form an alkaline hydrolysis environment, and the crystalline flake graphite is ZrOCl 2 ·8(H 2 O) hydrolysis to form ZrO 2 Providing a reaction basis.
The introduction of boron can induce graphite to form a three-dimensional network structure, so that the deformation of the material caused by thermal expansion and contraction can be relieved, and the thermal shock stability of the material can be improved. By hydrolysis of zirconium with ZrO 2 The particle form is doped into the graphite structure in situ, so that on one hand, the internal space of the graphite can be effectively increased, the specific surface area of the graphite is increased, the full contact between the graphite and other components is promoted, and the function maximization under the low-carbon premise is realized; on the other hand ZrO 2 The magnesium carbon brick has excellent rigidity and toughness and good thermal shock resistance, and can strengthen the stability of a graphite structure and reduce the oxidation rate of graphite when being doped in the graphite structure, thereby obtaining the magnesium carbon brick with low carbon, high thermal shock resistance and long service life.
It should be emphasized that, although the three-dimensional network structure of graphite has pores, the subsequent process of preparing magnesia carbon bricks and the actual application of magnesia carbon bricks will not result in the improvement of apparent porosity, but rather will exhibit a certain degree of reduction of apparent porosity, probably due to the following reason 2 The composite in the graphite structure effectively inhibits the oxidation of graphite, thereby inhibiting the formation of partial pores.
The SiC powder and the aluminum powder can be used as antioxidants in a synergistic way to inhibit oxidation phenomena in the preparation process and the use process of the magnesia carbon brick. Meanwhile, the SiC powder has the advantages of high strength, good thermal stability, good wear resistance and the like, and the uniform distribution of the SiC powder can play a role in strengthening brick bodies and improving mechanical properties.
Further, the mass ratio of ethylenediamine to ammonia water is 1:2-3, and the activation time is 5-6 hours.
Further, zrOCl in the modified solution 2 ·8(H 2 O), borate and deionized water at a ratio of 0.3mol:0.3mol:1000ml.
Further, the mass volume ratio of the activated crystalline flake graphite to the modified solution is 10-20 g/100 mL.
In step S2, the temperature of heating and stirring is 100 ℃, the time is 10-12 h, the drying temperature is 110-120 ℃, and the drying time is 7-8h.
Further, the MgO content of the fused magnesia is more than or equal to 97wt percent, and the volume density of the fused magnesia is more than or equal to 3.45g/cm 3 CaO and SiO in fused magnesia 2 The mass ratio of (2) is more than or equal to 2, and the granularity of the fused magnesia is less than 200 meshes.
Further, the purity of aluminum in the aluminum powder is more than 99wt percent, and the granularity is less than 200 meshes.
Further, the average granularity of the SiC powder is 100nm, and the SiC content is more than 99wt%.
Further, the phenolic resin is a thermosetting phenolic resin.
The second aspect of the invention provides a preparation method of the low-carbon magnesia carbon brick for the refining ladle, which comprises the following preparation steps:
ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
placing the mixed and ground material into a mould, and performing compression molding to obtain a brick blank;
and performing heat treatment on the green bricks to obtain the low-carbon magnesia carbon bricks for refining ladle.
Further, the mixture is pressed and molded under the condition of 150-200 MPa.
Further, heat treatment is carried out for 20-24 hours at the temperature of 200-240 ℃.
The beneficial effects obtained by one or more of the technical schemes of the invention are as follows:
the low-carbon magnesia carbon brick for refining ladle has volume density not less than 3.2 g/cm 3 The apparent porosity is less than or equal to 2.6 percent, and the normal-temperature compressive strength is more than or equal to 96.5MPa; the high-temperature flexural strength (1400 ℃ multiplied by 0.5 h) is more than or equal to 37.6 MPa, the thermal shock resistance times is more than or equal to 11, the slag resistance test (1400 ℃ multiplied by 0.5 h) does not see obvious erosion and penetration, the service life is more than 60 times, and the high-temperature thermal shock resistance test has high thermal shock resistance and long service life.
Detailed Description
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail below with reference to specific examples and comparative examples.
The materials used in the following examples and comparative examples are as follows:
(1) Electric smelting magnesite: the MgO content of the fused magnesia is more than or equal to 97wt percent, and the volume density of the fused magnesia is more than or equal to 3.45g/cm 3 CaO and SiO in fused magnesia 2 The mass ratio of (2) is more than or equal to 2, and the granularity of the fused magnesia is less than 200 meshes.
(2) Aluminum powder: the purity of the aluminum is more than 99 weight percent, and the granularity is less than 200 meshes.
(3) SiC powder: the average particle size is 100nm, and the SiC content is more than 99 weight percent.
(4) Phenolic resin: thermosetting phenolic resin.
Example 1
The embodiment provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 90 parts of fused magnesia, 10 parts of aluminum powder and 5 parts of boron doped ZrO 2 10 parts of SiC powder and 5 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Boron doped ZrO 2 Preparation of graphite composite material:
s1: mixing ethylenediamine and ammonia water in a mass ratio of 1:2, soaking crystalline flake graphite in a mixed solution of ethylenediamine and ammonia water for activation for 5 hours, filtering out crystalline flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O), borate and deionized water are mixed according to the proportion of 0.3mol:0.3mol:1000ml to form a modified solution; dispersing 10g of activated crystalline flake graphite in 100mL of the modified solution, heating and stirring for 12h at 100 ℃, filtering, washing with water, and drying for 7h at 110 ℃ to obtain boron doped ZrO 2 Graphite composite material;
(2) ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
(3) Placing the mixed and ground material into a mould, and pressing and forming under 150MPa to obtain a brick blank;
(4) Pushing the green bricks into a heat treatment kiln at 240 ℃ for heat treatment for 20 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Example 2
The embodiment provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 70 parts of fused magnesia, 5 parts of aluminum powder and 2 parts of boron doped ZrO 2 Graphite composite material, 5 parts of SiC powder and 3 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Boron doped ZrO 2 Preparation of graphite composite material:
s1: mixing ethylenediamine and ammonia water in a mass ratio of 1:3, soaking crystalline flake graphite in a mixed solution of ethylenediamine and ammonia water for activation for 6 hours, filtering out crystalline flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O), borate and deionized water are mixed according to the proportion of 0.3mol:0.3mol:1000ml to form a modified solution; dispersing 15g of activated crystalline flake graphite in 100mL of the modified solution, heating and stirring for 10h at 100 ℃, filtering, washing with water, and drying for 7h at 120 ℃ to obtain boron doped ZrO 2 Graphite composite material;
(2) ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
(3) Placing the mixed and ground material into a mould, and pressing and forming under 180MPa to obtain a brick blank;
(4) Pushing the green bricks into a heat treatment kiln at 200 ℃ for heat treatment for 24 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Example 3
The embodiment provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 80 parts of fused magnesia, 7 parts of aluminum powder and 3 parts of boron doped ZrO 2 Graphite composite material, 8 parts of SiC powder and 2 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Boron doped ZrO 2 Preparation of graphite composite material:
s1: mixing ethylenediamine and ammonia water in a mass ratio of 1:2, soaking crystalline flake graphite in a mixed solution of ethylenediamine and ammonia water for activation for 6 hours, filtering out crystalline flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O), borate and deionized water are mixed according to the proportion of 0.3mol:0.3mol:1000ml to form a modified solution; dispersing 20g of activated crystalline flake graphite in 100mL of the modified solution, heating and stirring for 11h at 100 ℃, filtering, washing with water, and drying for 8h at 110 ℃ to obtain boron doped ZrO 2 Graphite composite material;
(2) ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
(3) Placing the mixed and ground material into a mould, and pressing and forming under 200MPa to obtain a brick blank;
(4) Pushing the green bricks into a 220 ℃ heat treatment kiln for heat treatment for 20 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Example 4
The embodiment provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 60 parts of fused magnesia, 1 part of aluminum powder and 1 part of boron doped ZrO 2 Graphite composite material, 5 parts of SiC powder and 1 part of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Boron doped ZrO 2 Preparation of graphite composite material:
s1: mixing ethylenediamine and ammonia water in a mass ratio of 1:3, soaking crystalline flake graphite in a mixed solution of ethylenediamine and ammonia water for activation for 5 hours, filtering out crystalline flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O), borate and deionized water are mixed according to the proportion of 0.3mol:0.3mol:1000ml to form a modified solution; dispersing 18g of activated crystalline flake graphite in 100mL of the modified solution, heating and stirring for 10h at 100 ℃, filtering, washing with water, and drying for 8h at 120 ℃ to obtain boron doped ZrO 2 Graphite composite material;
(2) ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
(3) Placing the mixed and ground material into a mould, and pressing and forming under 150MPa to obtain a brick blank;
(4) Pushing the green bricks into a 230 ℃ heat treatment kiln for heat treatment for 22 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Comparative example 1
The comparative example provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 90 parts of fused magnesia, 10 parts of aluminum powder, 5 parts of crystalline flake graphite, 10 parts of SiC powder and 5 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Mixing and grinding fused magnesia, aluminum powder, crystalline flake graphite, siC powder and phenolic resin in proportion;
(2) Placing the mixed and ground material into a mould, and pressing and forming under 150MPa to obtain a brick blank;
(3) Pushing the green bricks into a heat treatment kiln at 240 ℃ for heat treatment for 20 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Comparative example 2
This comparative example provides a refining ladleThe low-carbon magnesia carbon brick is prepared from the following raw materials in parts by weight: 90 parts of fused magnesia, 10 parts of aluminum powder, 3 parts of crystalline flake graphite and 2 parts of ZrO 2 10 parts of SiC powder and 5 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
(1) Fused magnesite, aluminium powder, crystalline flake graphite and ZrO 2 Mixing and grinding the powder, siC powder and phenolic resin according to a certain proportion;
(2) Placing the mixed and ground material into a mould, and pressing and forming under 150MPa to obtain a brick blank;
(3) Pushing the green bricks into a heat treatment kiln at 240 ℃ for heat treatment for 20 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Comparative example 3
The comparative example provides a low-carbon magnesia carbon brick for a refining ladle, which comprises the following preparation raw materials in parts by mass: 90 parts of fused magnesia, 10 parts of aluminum powder and 5 parts of ZrO 2 10 parts of SiC powder and 5 parts of phenolic resin.
The preparation method of the low-carbon magnesia carbon brick for the refining ladle comprises the following steps:
（1）ZrO 2 preparation of graphite composite material:
s1: mixing ethylenediamine and ammonia water in a mass ratio of 1:2, soaking crystalline flake graphite in a mixed solution of ethylenediamine and ammonia water for activation for 5 hours, filtering out crystalline flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O) and deionized water are mixed according to the proportion of 0.3mol to 1000ml to form a modified solution; dispersing 10g of activated crystalline flake graphite in 100mL of the modified solution, heating and stirring at 100deg.C for 12h, filtering, washing with water, and drying at 110deg.C for 7h to obtain ZrO 2 Graphite composite material;
(2) Fused magnesia, aluminum powder and ZrO are mixed 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
(3) Placing the mixed and ground material into a mould, and pressing and forming under 150MPa to obtain a brick blank;
(4) Pushing the green bricks into a heat treatment kiln at 240 ℃ for heat treatment for 20 hours, and obtaining the low-carbon magnesia carbon bricks for refining steel ladles.
Performance test:
the magnesia carbon bricks prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests, wherein the indexes of the tests comprise volume density, apparent porosity, normal-temperature compressive strength, high-temperature flexural strength of carbon implantation (1400 ℃ C. X0.5 h), and thermal shock resistance times (according to the national standard of the magnesia carbon brick thermal shock resistance test, namely, 950 ℃ C. Heat treatment and air cooling, then 0.3MPa pressure is applied, the sample is not destroyed, the next thermal shock resistance test is performed, the thermal shock resistance performance characterization is performed according to the thermal shock resistance times), and slag erosion and penetration phenomena and service life are performed in the slag resistance test under the carbon implantation atmosphere of 1400 ℃ C. Heat preservation for 0.5h, and the specific results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the low carbon magnesia carbon bricks for refining ladle provided by examples 1 to 4 of the present invention have a bulk density of 3.2. 3.2 g/cm or more 3 The apparent porosity is less than or equal to 2.6 percent, and the normal-temperature compressive strength is more than or equal to 96.5MPa; the high-temperature flexural strength (1400 ℃ multiplied by 0.5 h) is more than or equal to 37.6 MPa, the thermal shock resistance times is more than or equal to 11, the slag resistance test (1400 ℃ multiplied by 0.5 h) does not see obvious erosion and penetration, the service life is more than 60 times, and the thermal shock resistance stability and the long service life are excellent.
The crystalline flake graphite in the low-carbon magnesia carbon brick of the comparative example 1 is not modified, is easy to generate an elastic effect in the direction parallel to the forming pressure of the brick body, causes internal stress concentration of the brick body, is easy to oxidize, causes surface layer tissue degradation of the brick body, reduces erosion resistance and stripping resistance of the brick body, ensures poor compressive strength, breaking strength and thermal shock stability of the brick body, and has short service life. In the low carbon type carbon magnesia carbon brick of comparative example 2, the crystalline flake graphite was not modified, but ZrO was additionally added 2 Powder, test results show ZrO 2 Although the performance is improved to a certain extent, the magnesia carbon brick still has slight slag erosion and penetration, compressive strength and fracture resistanceThe strength and thermal shock stability are still unsatisfactory. In the low carbon type carbon magnesia carbon brick of comparative example 3, the crystalline graphite is ZrO 2 The modification is carried out without introducing boron into the graphite, so that a stable three-dimensional network structure is difficult to obtain, the internal space of the graphite is small, the material can deform due to thermal expansion and contraction, and the material is in insufficient contact with other components, so that the thermal shock stability and the service life of the material are poor.
Claims (10)
1. A refining ladle is with low carbon formula magnesia carbon brick which characterized in that: the preparation raw materials comprise the following components in parts by weight: 60-90 parts of fused magnesia, 1-10 parts of aluminum powder and 1-5 parts of boron doped ZrO 2 5-10 parts of SiC powder and 1-5 parts of phenolic resin;
boron doped ZrO 2 The preparation method of the graphite composite material comprises the following steps:
s1: soaking the flake graphite in a mixed solution of ethylenediamine and ammonia water for full activation, filtering the flake graphite, and drying;
s2: zrOCl 2 ·8(H 2 O) and borate are dissolved in deionized water to form a modified solution; dispersing activated crystalline flake graphite in the modified solution, heating and stirring, filtering, washing with water, and drying to obtain boron doped ZrO 2 Graphite composite material.
2. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: the mass ratio of the ethylenediamine to the ammonia water is 1:2-3, and the activation time is 5-6 hours.
3. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: zrOCl in the modified solution 2 ·8(H 2 O), borate and deionized water in the addition ratio of 0.3mol:0.3mol:1000ml;
the mass volume ratio of the activated crystalline flake graphite to the modified solution is 10-20 g/100 mL.
4. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: in the step S2, the heating and stirring temperature is 100 ℃, the time is 10-12 h, the drying temperature is 110-120 ℃, and the drying time is 7-8h.
5. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: the MgO content of the fused magnesia is more than or equal to 97wt percent, and the volume density of the fused magnesia is more than or equal to 3.45g/cm 3 CaO and SiO in fused magnesia 2 The mass ratio of (2) is more than or equal to 2, and the granularity of the fused magnesia is less than 200 meshes.
6. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: the purity of aluminum in the aluminum powder is more than 99 weight percent, and the granularity is less than 200 meshes.
7. The low carbon magnesia carbon brick for a refining ladle as claimed in claim 1, wherein: the average granularity of the SiC powder is 100nm, and the SiC content is more than 99wt%;
the phenolic resin is thermosetting phenolic resin.
8. The method for preparing the low-carbon magnesia carbon brick for the refining ladle as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
ZrO doping fused magnesite, aluminum powder and boron 2 Mixing and grinding the graphite composite material, siC powder and phenolic resin according to a certain proportion;
placing the mixed and ground material into a mould, and performing compression molding to obtain a brick blank;
and performing heat treatment on the green bricks to obtain the low-carbon magnesia carbon bricks for refining ladle.
9. The method for preparing the low-carbon magnesia carbon brick for the refining ladle as claimed in claim 8, wherein the method comprises the following steps: and (5) pressing and forming under the condition of 150-200 MPa.
10. The method for preparing the low-carbon magnesia carbon brick for the refining ladle as claimed in claim 8, wherein the method comprises the following steps: and heat-treating for 20-24 hours at the temperature of 200-240 ℃.
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